CN101225126A - Method for extracting chitin and chitin thereof - Google Patents
Method for extracting chitin and chitin thereof Download PDFInfo
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- CN101225126A CN101225126A CNA2008100577371A CN200810057737A CN101225126A CN 101225126 A CN101225126 A CN 101225126A CN A2008100577371 A CNA2008100577371 A CN A2008100577371A CN 200810057737 A CN200810057737 A CN 200810057737A CN 101225126 A CN101225126 A CN 101225126A
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Abstract
The invention provides a method to extract a chitin by utilizing the residue of a cochineal insect from which a haematochrome is already extracted and a chitin prepared by the method. The chitin extraction method comprises: 1) the residue of the cochineal is hydrolyzed and the protein is deprived, 2) the inorganic salt inside the residue is removed and a crude product of the chitin is derived from the residue, 3) an oxidant is added into the crude product of the chitin to do the oxidation and the decoloration process. The extraction method is characterized in that taking use of the residue of the cochineal from which the haematochrome is extracted as a raw material with simple process and easy operation, the prepared chitin appearance color and lustre and physiochemical index are in accordance with the standards for the food, medicine, cosmetics, agriculture, and environment protection, and the prepared chitin by the method is possessed of high purity and low ash content. The extraction and preparation method of the chitin from the residue of a cochineal insect has the advantages of utilizing comprehensively the resource, achieving the purpose of full use of the whole cochineal insect, decreasing the environmental pollution, and improving the economic profit for the enterprises.
Description
Technical field
The present invention relates to a kind of extracting method of organic high molecular compound, be specifically related to a kind of extracting method of natural macromolecule amylose and the natural macromolecule amylose of extraction thereof.
Background technology:
Chitin (Chitin) has another name called chitin, chitin, chitin, glutelin, bright angle glutelin, chitin, crab shell chitosan, insoluble chitin etc., and chemistry is by name poly-, and β-(1,4)-2-acetamido-2-deoxy-D-glucose molecular formula is (C
8H
15NO
6) n, be the unique natural alkaline polysaccharide of finding so far.Chitin extensively is present in the shrimp of Arthropoda Crustacea animal, the crust of crab, and chitin content is 20%～25% in its Prawn shell, and the content in the crab shell is between 15%～20%; The crust of Insecta (as Coleoptera, Diptera wing etc.), mollusk (shellfish) cuttlefish skeleton, in the cell walls of Mycophyta lower plant such as yeast, fungal hyphae cell and alga cells and higher plant (as mushroom), in the standing stock natural organic-compound on earth, be only second to Mierocrystalline cellulose, being second largest renewable resources on the earth, also is the nitrogenous natural organic-compound of the outer quantity maximum of isolating protein on the earth, estimates 10,000,000,000 tons of nature year biosynthesizing amounts nearly.In vivo, chitin exists with the protein-polysaccharide form and polypeptide, calcareous, pigment etc. combine.
Since professor H.Braconnot of France in 1811 finds chitin (Chitin), the research history of chitin and derivative thereof reaches nearly 200 years, but it becomes the front subject field that is caught people's attention deeply gradually, by the numerous scientists in the world are studied, is the thing of nearly decades.In recent years, the chitin of natural animal extraction (particularly insect) has all obtained using widely in foodstuff production, medicine, industry etc.Studies show that, the physics of chitin and chemical property are stable, certain intensity is arranged, also has Biodegradable in addition, can be decomposed by the intravital N,O-Diacetylmuramidase of biology, good with the affinity of organism, nontoxic, has good water absorbability, film-forming properties, gas permeability, biocompatibility, thereby in medical science, agroforestry, functional materials, light and textile industries, field such as environmental protection and food is widely used, have crucial utility value and economic worth, be described as " human the 6th vital principle ", " 21 century is the century of chitin ", " 21 century STUDY ON POLYSACHAROSE most promising be chitin ", " main flow material-chitin of 21 century " etc. we can say that chitin will be one of lofty perch of 21 century high and new technology competition.The present main raw material that is used for the suitability for industrialized production chitin both at home and abroad is shrimp, crab shell.In recent years, the report of chitin extraction from insect is arranged, but this respect research is also fewer.
Chitin belongs to the water-insoluble polysaccharide compounds, and is similar to cellulosic structure.Through structural analysis, chitin is the unique positively charged a kind of natural polymers of occurring in nature, belongs to the straight chain glycosaminoglycan, and molecular formula is (C
8H
13NO
5)
n, connecting with β (1 → 4) glycosidic bond between the monomer, molecular weight is generally 10
6About, theoretical nitrogen content 6.9%.Its molecular structure characteristics are: Sauerstoffatom is connected to the sugar ring of each carbon atom on the next sugar ring, and pendant groups " extension " is on these rings.The cellulosic molecular structure of chemistry that extensively exists in the molecular structure of chemistry of chitin and the plant is respectively:
This shows that chitin molecule chemical structure and plant cellulose are closely similar, different is, if a hydroxyl of forming on second carbon atom of cellulosic individual molecule-glucose molecule (OH) changes acetamido (NHCOCH into
3), Mierocrystalline cellulose has just become chitin like this, and in this sense, chitin can be described as animal fiber.
Chitin is white in color or canescence; unformed translucent chip solid; because strong hydrogen bond action between macromole; cause chitin to become the biological a kind of structural material of protection, crystal structure is firm, does not generally melt; also water insoluble, diluted acid, diluted alkaline, concentrated base and common organic solvents; but dissolve in dense hydrochloric acid, sulfuric acid, phosphoric acid and anhydrous formic acid, main chain is degraded simultaneously, and viscosity reduces.Chitin chemistry character is highly stable, if the acetamido of sloughing in the molecule just can be converted into soluble chitin (Chitosan), or claims chitosan (shell polyamine, chitosan), and it is the most important derivative of chitin.Chitosan is good than the chitin solvability, thereby its range of application also just becomes very wide, in fields such as medicine, agricultural, industry, makeup, environment protection, water treatments purposes is extremely widely arranged.
In health care, with the absorption-type surgical sewing thread softness that chitin is made, the physical strength height is easily absorbed by body, does not change the content of oxyproline in the skin collagen simultaneously, NIP reaction, also available ordinary method sterilization.The medical dressing that chitin and chitin fiber are made has non-woven, gauze, bandage, hemostatic cotton etc., is mainly used in treatment burn patient.Chitosan and chitin also are the ideal materials of making artificial skin, chitin/chitosan artificial skin quality softness, comfortable is good with the coating performance of the surface of a wound, not only ventilative but also absorb water, the inhibiting bacteria and diminishing inflammation effect is not only arranged, and have the function of inhibition of pain, hemostasis and promotion wound healing.Chitin can be used as cigarette tackiness agent and objectionable constituent sorbent material, reduces objectionable constituent content greatly, improves cigarette fragrance, improves the cigarette class.
In foodstuff manufacturing, the derivative of chitin/chitosan as the new type functional food additive, is widely used in foodstuffs industry, has to preserve moisture, seasoning, improve Food Quality, effect such as anticorrosion.Chitin/chitosan belongs to the natural sex material, has no side effect.Chitin and derivative thereof can also be used as thickening material, emulsifying agent, weighting agent, stablizer, discoloring agent, the fixation support of fragrance enriching substance, water-holding agent, enzyme and the organic floculant of food industrial wastewater etc.
On agricultural, chitin and derivative thereof have adequate stability, as using in soil, can change soil microflora: promote actinomycetes and the growth of some other beneficial microorganism thereof in the soil, suppress pathogenic bacteria growth and breeding in the soil; Can also improve the crumb structure of soil effectively; As be sprayed onto soil surface, and can form thin film, have the soil moisture conservation effect; Also agricultural chemicals or chemical fertilizer can be mixed wherein, make their uniform mixing, obtain the effect of slowly-releasing.Many chitin and derivatives thereof of studies show that also can be used as a kind of novel plant-growth regulator, can excite seed germination, promote plant growth, increase output, improve quality.Chitin and derivative thereof can also be used as Plant diseases resistance inductor, drought resistance agent or water-holding agent, fruit and vegetable fresh-keeping agent, fodder additives and farm chemical carrier etc. in addition.
In wastewater treatment, chitin is chitosan particularly, owing to have-NH in the molecule
2,-OH is a natural polymeric chelant, can be from solution trap heavy metals effectively.
On daily cosmetics, the chitin powder is a dry cleaning composition ideal activity material, and its specific surface area is big, and the porosity height can absorb the sebum quasi-grease, and its ability that absorbs sebum is much larger than starch or other active substance.
Cochineal (Cochineal insects) is meant a class scale insect of female worm energy production cochineal pigment, belong to the Dactylopius coccus Costa cochineal (Cochineal) that Homoptera (Homoptera) mealybug Superfamily (Pseudococcoidea) fuchsin a red-spotted lizard section (Dctylopiidae) fuchsin a red-spotted lizard belongs to (Dactylopius), originate in Mexico and Central and South America, the host is a cactus plant.People utilize the cochineal stem body to extract the cochineal pigment for a long time, be widely used in multiple industries such as food, makeup, medicine, for example, extract the haematochrome technological process below the employing usually from cochineal, comprise: 1) remove ester matter: 100 gram cochineal stem bodys add 400 milliliters of sherwood oils, reflux kept constant temperature, slight boiling condition about 6 hours, then filtered while hot; Add 400 milliliters of dehydrated alcohols in the polypide container is housed again, reflux kept constant temperature, slight boiling condition about 6 hours, and filtered while hot must be removed the cochineal stem body of ester matter; 2) remove pigment: in the container that the cochineal stem body of removing ester matter is housed, add 400 ml deionized water, be heated to 80～85 ℃, refluxed 4 hours, filtered while hot, filtrate is cochineal pigment solvent or diluent; 3) repeat the reflux lixiviate and get the polypide pigment totally eight times, filtered while hot, liquid-solid separation, the plain cochineal worm slag that obtains discoloring, the worm slag is the dark brown speckles shape, water ratio 82%, nitrogen content 37.31%, ash content 4.81%.The average content of chitin is 6.29% (in over dry worm slag) in the worm slag.Usually this cochineal worm slag is as the residuum depleted.
For example, the applying date is that March 23 calendar year 2001, the patent No. are to disclose a kind of " the cochineal colorant of purification and produce its method " in the Chinese patent of ZL01802714.8.This method is extracted the cochineal colorant from cochineal, by allowing cochineal extract solution carry out proteolysis, at least a processing of carrying out then in adsorption treatment, ion exchange treatment, acid treatment, extracting processing and the film processing is not less than 6000 fraction and obtains the cochineal colorant to remove molecular weight.This method has been extracted the cochineal colorant from the cochineal powder after, produce a large amount of residuum worm slags, these worm slags normally are used as refuse and handle, and do not obtain any utilization.
Summary of the invention
The objective of the invention is to provide a kind of method of chitin extraction at problems of the prior art; this method is utilized chitin extraction from the cochineal residuum worm slag behind the cochineal extraction haematochrome; the technology that adopts is simple and easy to operate; chitin appearance luster of being extracted and physical and chemical index meet the standard of industries such as being applied to food, medicine, makeup, agricultural and environment protection; and the ash content of chitin is low, yield and nitrogenous rate are higher; utilize natural resources fully, improved the business economic benefit.
For realizing the object of the invention, one aspect of the present invention provides a kind of method of chitin extraction, and the cochineal worm slag that employing is extracted behind the cochineal pigment is a raw material, and the step process worm slag that carries out in the following order obtains chitin: 1) remove the protein in the worm slag; 2) inorganic salt in the removal worm slag obtain the chitin crude product; 3) in the chitin crude product, add oxygenant and carry out oxidative decoloration, obtain chitin.
In addition, also comprise step 4): filter and dry, will filter, wash by the chitin crude product behind the described oxidative decoloration filter residue until washing fluid for neutral, be drying to obtain the chitin finished product.
Wherein, in step 1), alkali lye is added in the worm slag, and with the mixture heating up of worm slag and alkali lye to 70-90 ℃, preferred 80 ℃, stirring reaction is more than 1 hour, preferred 1-3 hour, be preferably 2 hours, filter then, till filtrate is neutrality with an amount of distilled water flushing to washing fluid, so that remove protein in the described worm slag.It is sodium hydroxide solution or the potassium hydroxide solution of 1.0-2.0mol/L that used alkali lye can be selected concentration, preferred 1.0mol/L.
Particularly, in step 1), the ratio of the weight (dry weight) of the volume of alkali lye and worm slag is 1-7: 1, and preferred 4: 1, i.e. worm slag weight (dry weight) 1g, then the volume of alkali lye is 1-7ml or worm slag weight (dry weight) 1kg, then the volume of alkali lye is 1-7L.
Wherein, in step 2) in, to add hydrochloric acid soln in the worm slag after step 1) removes protein, and make mixture be warming up to 50-70 ℃, preferred 50 ℃, reaction is more than 0.5, preferred reaction 0.5-1.5 hour, preferably reacted 1 hour, filter then, till filtrate is neutrality with an amount of distilled water flushing to washing fluid, so that remove inorganic salt in the described worm slag.The concentration of used salt acid solution is 1.0-3.0mol/L, preferred 1.0mol/L.
Particularly, in step 2) in, the ratio of the weight (dry weight) of the volume of hydrochloric acid soln and worm slag is 1-7: 1, preferred 4: 1, be worm slag weight (dry weight) 1g, then the volume of hydrochloric acid soln is 1-7ml or worm slag weight (dry weight) 1Kg, and then the volume of hydrochloric acid soln is 1-7L.
Wherein, the oxidative decoloration of step 3) is handled and is comprised: at first will be through step 2 with dispersion agent) the chitin crude product that obtains is dispersed into suspension; then in suspension, add complexing agent and carry out complex reaction; add stablizer and protective material then; adding oxygenant at last decolours; bleaching time is 20-40 minute, preferred 30 minutes.
Wherein, dispersion agent is a deionized water, and the weight of dispersion agent is 6-12 times of described chitin crude product weight (dry weight), preferred 9 times; Complexing agent is selected diethylene triamine pentacetic acid (DTPA) (DTPA), and its weight is the 0.05-0.2% of chitin crude product weight (dry weight), and preferred 0.1%; Stablizer is selected water glass, and consumption is the 1-5% of chitin crude product weight (dry weight), is preferably 3%; Protective material is selected manganous sulfate, and consumption is the 0.1-1% of chitin crude product weight (dry weight), is preferably 0.5%; It is the superoxol of 5-20% that oxygenant is selected concentration, and preferred concentration is 10% superoxol, and the oxygenant consumption is the 1-10% of chitin crude product weight (dry weight), preferred 6%.
Particularly, the time that chitin crude product suspension carries out complex reaction is 5-20 minute, preferred 10 minutes.
Another aspect of the present invention provides a kind of chitin that extracts from cochineal, it is characterized in that being formed by method for preparing.
Adopt the advantage of the chitin of the inventive method extraction to be:
The inventive method is that raw material extracts refining chitin with the residuum worm slag that extracts behind the haematochrome; the yield height of chitin not only; the nitrogen content height; ash oontent is low; impurity is few; the capability and performance index satisfies the standard of industries such as food, medicine, makeup, agricultural and environment protection; and the residuum worm slag behind original cochineal extraction haematochrome is effectively used; thereby utilize resources synthetically has improved comprehensive utilization of resources value; reduced the production cost of chitin; reduce environmental pollution, helped environment protection.
Brief Description Of Drawings
The extraction process schema of Fig. 1 chitin
The infrared spectrogram of Fig. 2 chitin standard specimen and cochineal worm slag chitin extraction sample
Embodiment
With the cochineal worm slag that extracted behind the cochineal pigment is the raw material chitin extraction, and the cochineal worm slag of removing pigment is the dark brown speckles shape, water ratio 82%, nitrogen content 37.31%, ash content 4.81%.The average content of chitin is 6.29% (in over dry worm slag) in the worm slag.
Embodiment 1
According to following steps chitin extraction from cochineal worm slag:
1) removes protein
Get cochineal worm slag 50g (dry weight), adding concentration is the sodium hydroxide solution 200mL of 1.0mol/L, heated and stirred mixes it, be heated to 80 ℃, react after 1 hour, adopt 200 purpose strainer filtering reaction solutions, with an amount of distilled water flushing of the filtrate of gained, the distilled water after flushing is neutral.
2) remove inorganic salt
Adding concentration in filtrate is 1.0mol/L hydrochloric acid 200mL, is heated to 50 ℃, and constant temperature stirs, lixiviate 60 minutes adopts 200 purpose filter screens to filter, with an amount of distilled water flushing filtrate, distilled water after flushing is neutral, and the filtrate of acquisition is the chitin crude product.
3) oxidative decoloration
Add the dispersion agent deionized water in the chitin crude product, the weight of deionized water is 9 times of chitin crude product weight, stirs then to make the chitin crude product be dispersed into suspension;
Then, adding weight in suspension is the complexing agent diethylenetriamine pentaacetic acid (DTPA) of chitin crude product weight (butt) 0.1%, stirs, and normal temperature reacted 10 minutes down;
Then, add stablizer water glass (Na
2SiO
3) and protective material manganous sulfate (MeSO
4) it is mixed, wherein, the weight of stablizer is 3% of chitin crude product weight (butt); The weight of manganous sulfate is 0.5% of chitin crude product weight (butt).
At last, adding concentration is 10% hydrogen peroxide (H
2O
2) solution, the weight of superoxol is 6% of chitin crude product weight (butt), slowly stirs, and decolours 30 minutes.
4) filtration drying
With the chitin crude product suspension behind the decoloring reaction with 200 purpose strainer filterings, the gained filter residue is with an amount of distilled water wash, until washings is neutral, with filter residue and drying, drying temperature is 100 ℃, dried water ratio is 0.7%, promptly obtains finished product chitin 2.765g, and the yield of chitin is 87.92% (in chitin content in the worm slag).
The capability and performance index detected result of chitin sees Table 1.
Embodiment 2
According to following steps chitin extraction from cochineal worm slag:
1) removes protein
Get cochineal worm slag 50g (dry weight), adding concentration is the sodium hydroxide solution 350mL of 2.0mol/L, heated and stirred mixes it, be heated to 90 ℃, react after 3 hours, adopt 200 purpose strainer filtering reaction solutions, with an amount of distilled water flushing of gained filtrate, the distilled water after flushing is neutral.
2) remove inorganic salt
Adding concentration in filtrate is 2.0mol/L hydrochloric acid 200mL, is heated to 60 ℃, and constant temperature stirs, and lixiviate 60 minutes adopts 200 purpose filter screens to filter, and with an amount of distilled water flushing filtrate, the distilled water after flushing is neutral, obtains the chitin crude product.
3) oxidative decoloration
To add the dispersion agent deionized water in the chitin crude product, the weight of deionized water is 6 times of chitin crude product weight, stirs then to make the chitin crude product be dispersed into suspension;
Then, adding weight in suspension is the complexing agent diethylenetriamine pentaacetic acid (DTPA) of chitin crude product weight (butt) 0.1%, stirs, and normal temperature reacted 20 minutes down;
Then, add stablizer water glass (Na
2SiO
3) and protective material manganous sulfate (MeSO
4) it is mixed, wherein, the consumption of stablizer is 5% of a chitin crude product weight (butt); The consumption of manganous sulfate is 1.0% of a chitin crude product weight (butt).
At last, adding concentration is 10% hydrogen peroxide (H
2O
2) solution, the weight of superoxol is 10% of chitin crude product weight (butt), slowly stirs, and decolours 20 minutes.
4) filtration drying
With the chitin crude product suspension behind the decoloring reaction with 200 purpose strainer filterings, the gained filter residue is with an amount of distilled water wash, until washings is neutral, with filter residue and drying, drying temperature is 100 ℃, dried water ratio is 0.7%, promptly obtains finished product chitin 2.115g, and the yield of chitin is 67.25% (in chitin content in the worm slag).
The capability and performance index detected result of chitin sees Table 1.
Embodiment 3
According to following steps chitin extraction from cochineal worm slag:
1) removes protein
Get cochineal worm slag 50g (dry weight), adding concentration is the sodium hydroxide solution 150mL of 1.5mol/L, heated and stirred mixes it, be heated to 70 ℃, react after 2 hours, adopt 200 purpose strainer filtering reaction solutions, with an amount of distilled water flushing of gained filtrate, the distilled water after flushing is neutral.
2) remove inorganic salt
Adding concentration in filtrate is 3.0mol/L hydrochloric acid 150mL, is heated to 70 ℃, and constant temperature stirs, and lixiviate 30 minutes adopts 200 purpose filter screens to filter, and with an amount of distilled water flushing filtrate, the distilled water after flushing is neutral, obtains the chitin crude product.
3) oxidative decoloration
To add the dispersion agent deionized water in the chitin crude product, the weight of deionized water is 12 times of chitin crude product weight, stirs then to make the chitin crude product be dispersed into suspension;
Then, adding weight in suspension is the complexing agent diethylenetriamine pentaacetic acid (DTPA) of chitin crude product weight (butt) 0.2%, stirs, and normal temperature reacted 5 minutes down;
Then, add stablizer water glass (Na
2SiO
3) and protective material manganous sulfate (MeSO
4) it is mixed, wherein, the consumption of stablizer water glass is 1% of a chitin crude product weight (butt); The consumption of manganous sulfate is 0.1% of a chitin crude product weight (butt).
At last, adding concentration is 10% hydrogen peroxide (H
2O
2) solution, the weight of superoxol is 1% of chitin crude product weight (butt), slowly stirs, and decolours 40 minutes.
4) filtration drying
With the chitin crude product suspension behind the decoloring reaction with 200 purpose strainer filterings, the gained filter residue is with an amount of distilled water wash, until washings is neutral, with filter residue and drying, drying temperature is 100 ℃, dried water ratio is 0.7%, promptly obtains finished product chitin 2.375g, and the yield of chitin is 75.52% (in chitin content in the worm slag).
The capability and performance index detected result of chitin sees Table 1.
Embodiment 4
According to following steps chitin extraction from cochineal worm slag:
1) removes protein
Get cochineal worm slag 50g (dry weight), adding concentration is the potassium hydroxide solution 300mL of 1.0mol/L, heated and stirred mixes it, be heated to 80 ℃, react after 2 hours, adopt 200 purpose strainer filtering reaction solutions, gained is crossed an amount of distilled water flushing of filtrate, the distilled water after flushing is neutral.
2) remove inorganic salt
Adding concentration in filtrate is 1.0mol/L hydrochloric acid 200mL, is heated to 50 ℃, and constant temperature stirs, and lixiviate 60 minutes adopts 200 purpose filter screens to filter, and with an amount of distilled water flushing filtrate, the distilled water after flushing is neutral, obtains the chitin crude product.
3) oxidative decoloration
To add deionized water in the chitin crude product, the weight of deionized water is 9 times of chitin crude product weight, stirs then to make the chitin crude product be dispersed into suspension;
Then, adding weight in suspension is the complexing agent diethylenetriamine pentaacetic acid (DTPA) of chitin crude product weight (butt) 0.1%, stirs, and normal temperature reacted 10 minutes down;
Then, add stablizer water glass (Na
2SiO
3) and protective material manganous sulfate (MeSO
4) it is mixed, wherein, the consumption of stablizer water glass is 3% of a chitin crude product weight (butt); The consumption of manganous sulfate is 0.5% of a chitin crude product weight (butt).
At last, adding concentration is 10% hydrogen peroxide (H
2O
2) solution, the weight of superoxol is 6% of chitin crude product weight (butt), slowly stirs, and decolours 30 minutes.
4) filtration drying
With the chitin crude product suspension behind the decoloring reaction with 200 purpose strainer filterings, the gained filter residue is with an amount of distilled water wash, until washings is neutral, with filter residue and drying, drying temperature is 100 ℃, dried water ratio is 0.7%, promptly obtains finished product chitin 2.455g, and the yield of chitin is 78.06% (in chitin content in the worm slag).
The capability and performance index detected result of chitin sees Table 1.
Experimental example 1
The chitin that extracts among the embodiment of the invention 1-4 is carried out the detection of nitrogen content, ash content, water ratio, and detected result sees Table 1.
Wherein, adopt Kjeldahl determination to measure the nitrogen content of chitin, the instrument that uses goes on foot the semi-automatic azotometer of B-324 type that outstanding company produces as Switzerland; " mensuration of ash content in the GB/T 5009.4-2003 food " method of employing is measured the ash content of chitin; The HR83 halogen moisture content tester that adopts plum Teller-Tuo benefit Instr Ltd. to produce is measured the water ratio of chitin.
Table 1 chitin quality examination result
| Outward appearance | Yield (%) | Nitrogen content (%) | Ash content (%) | Water ratio (%) | |
| Embodiment 1 | White or canescence, sheet | 87.92 | 4.66 | 0.72 | 0.7 |
| Embodiment 2 | 67.25 | 3.80 | 0.08 | 0.7 | |
| Embodiment 3 | 75.52 | 4.04 | 0.01 | 0.7 | |
| Embodiment 4 | 78.06 | 4.46 | 0.67 | 0.7 |
Experimental result shows, uses the inventive method chitin extraction, and the yield height of chitin reaches more than 67.25% (in the chitin content in the worm slag); Adopt the inventive method purified chitin purity height, the nitrogen content height reaches 3.80～4.66%, and ash content is low, reaches 0.01～0.72%, and water ratio is low, reaches 0.7%.According to the chitin that the inventive method is extracted, its refining effect is remarkable.
With shrimp shell, crab shell is the quality standard such as the table 2 of the chitin of raw material extraction
| Rank | Outward appearance | Moisture content | Ash | Nitrogen content |
| Food grade | Color prime white | ≤10％ | ≤1.0％ | 6.2-6.9％ |
| Technical grade | Canescence | ≤12％ | ≤2.0％ | - |
(shrimp, crab chitin quality standard that Jinan Haidebei Marine Organism Engineering Co., Ltd. produces)
Contrast embodiment of the invention 1-4 product and be the capability and performance index of the chitin that extracts of raw material, the chitin yield and the nitrogen content height that extract of the inventive method as can be seen with shrimp shell, crab shell; Ash content and water ratio are low, and the chitin of the inventive method preparation reaches the quality standard of technical grade chitin in the market.Therefore the chitin of the inventive method extraction can substitute the chitin in other sources in the market.
Experimental example 2
The chitin sample of getting the present invention's preparation carries out infrared spectra and detects, and adopts the FTS-40 Fourier transformation infrared spectrometer of the U.S. one hundred happy company to carry out infrared spectra detection, the resolving power of this instrument: RES=8, scanning times: SCANS=16.The chitin standard specimen is bought from Sigma company.
The chitin results of IR is seen Fig. 2.
The infrared spectra detected result shows: the chitin and the chitin standard specimen spectrogram principal character peak of the inventive method preparation match: be O-H stretching vibration absorption peak near 3400cm～1, it near 3264cm～1 N-H stretching vibration absorption peak, 3 peaks in 2962cm～1～2890cm～1 scope are C-H stretching vibration absorption peaks, 1652cm～1, near 3 peaks 1555cm～1 and 1310cm～1 are respectively acid amides I, II, III bands of a spectrum (chitin charateristic avsorption band), 4 peaks in 1070cm～1～1020cm～1 scope are C-O stretching vibration absorption peaks, are ring stretching vibration absorption peak near 890cm～1.
Claims (10)
1. the method for a chitin extraction, adopting cochineal worm slag is raw material, comprises following step in sequence: 1) remove the protein in the worm slag; 2) inorganic salt in the removal worm slag obtain the chitin crude product; 3) in the chitin crude product, add oxygenant and carry out oxidative decoloration.
2. the method for claim 1 is characterized in that: in described step 1), add alkali lye so that remove protein in the described worm slag in described worm slag.
3. method as claimed in claim 2 is characterized in that: described alkali lye is sodium hydroxide solution or potassium hydroxide solution, and concentration is 1.0-2.0mol/L.
4. as claim 2 or 3 described methods, it is characterized in that: to temperature 70-90 ℃, reaction is more than 1 hour with the mixture heating up of described worm slag and alkali lye.
5. the method for claim 1 is characterized in that: in described step 2) in, in described worm slag, adding hydrochloric acid soln so that remove described inorganic salt, the concentration of described hydrochloric acid soln is 1.0-3.0mol/L.
6. method as claimed in claim 5 is characterized in that: to 50-70 ℃, reaction is more than 0.5 hour with the mixture heating up of described worm slag and hydrochloric acid soln.
7. the method for claim 1; it is characterized in that: in described step 3): at first described chitin crude product is dispersed into suspension with dispersion agent; then in suspension, add intercalating agent and carry out complex reaction; add stablizer and protective material then, add described oxygenant at last and carry out described decolouring.
8. method as claimed in claim 7 is characterized in that: described dispersion agent is a deionized water, and described intercalating agent is selected diethylene triamine pentacetic acid (DTPA) (DTPA), and described stablizer is selected water glass, and described protective material is selected manganous sulfate; It is the superoxol of 5-20% that described oxygenant is selected concentration.
9. method as claimed in claim 8 is characterized in that: the consumption of described dispersion agent is 6-12 a times of described chitin crude product dry weight; The consumption of described intercalating agent is the 0.05-0.2% of chitin crude product dry weight; Described stablizer and protectant consumption are respectively the 1-5% and the 0.1-1% of chitin crude product dry weight, and the consumption of described oxygenant is the 1-10% of chitin crude product dry weight.
10. a chitin is characterized in that being prepared from according to the arbitrary described method of claim 1～9.
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| CN2008100577371A CN101225126B (en) | 2008-02-14 | 2008-02-14 | Method for extracting chitin and chitin thereof |
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| CN101225126B CN101225126B (en) | 2011-08-31 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276758A (en) * | 2011-08-10 | 2011-12-14 | 绵阳师范学院 | Method for comprehensively utilizing insect Chinese medicine dregs |
| CN102372795A (en) * | 2010-08-25 | 2012-03-14 | 浙江科技学院 | Method for preparing beta-chitin by utilizing squid theca |
| CN107410462A (en) * | 2017-04-09 | 2017-12-01 | 湖南易科生物工程有限公司 | A kind of compound method of leaf vegetables antistaling agent |
| CN109001470A (en) * | 2018-09-30 | 2018-12-14 | 南京财经大学 | A kind of precise determination method of protein content in edible mushroom |
| WO2019179148A1 (en) * | 2018-03-19 | 2019-09-26 | 扬州日兴生物科技股份有限公司 | Method for preparing glucosamine by using shrimp and crab shells as raw materials |
| CN115232228A (en) * | 2022-08-04 | 2022-10-25 | 中国科学院海洋研究所 | Method for extracting chitin from sea cockroach |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094944C (en) * | 1999-09-15 | 2002-11-27 | 天津大学 | Process for preparing chitosan |
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2008
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372795A (en) * | 2010-08-25 | 2012-03-14 | 浙江科技学院 | Method for preparing beta-chitin by utilizing squid theca |
| CN102372795B (en) * | 2010-08-25 | 2014-04-09 | 浙江科技学院 | Method for preparing beta-chitin by utilizing squid theca |
| CN102276758A (en) * | 2011-08-10 | 2011-12-14 | 绵阳师范学院 | Method for comprehensively utilizing insect Chinese medicine dregs |
| CN102276758B (en) * | 2011-08-10 | 2013-07-03 | 绵阳师范学院 | Method for comprehensively utilizing insect Chinese medicine dregs |
| CN107410462A (en) * | 2017-04-09 | 2017-12-01 | 湖南易科生物工程有限公司 | A kind of compound method of leaf vegetables antistaling agent |
| WO2019179148A1 (en) * | 2018-03-19 | 2019-09-26 | 扬州日兴生物科技股份有限公司 | Method for preparing glucosamine by using shrimp and crab shells as raw materials |
| CN109001470A (en) * | 2018-09-30 | 2018-12-14 | 南京财经大学 | A kind of precise determination method of protein content in edible mushroom |
| CN115232228A (en) * | 2022-08-04 | 2022-10-25 | 中国科学院海洋研究所 | Method for extracting chitin from sea cockroach |
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| CN101225126B (en) | 2011-08-31 |
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